1、Designation: D5075 01 (Reapproved 2017)1Standard Test Method forNicotine and 3-Ethenylpyridine in Indoor Air1This standard is issued under the fixed designation D5075; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of las
2、t revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEReapproved with editorial changes throughout in March 2017.1. Scope1.1 This test method covers the sampling/analysis of nico-tin
3、e and 3-ethenylpyridine (3-EP) in indoor air. This testmethod is based upon the collection of nicotine and 3-EP byadsorption on a sorbent resin, extraction of nicotine and 3-EPfrom the sorbent resin, and determination by gas chromatog-raphy (GC) with nitrogen selective detection. (1)21.2 The active
4、samplers consist of an macroreticularpolystyrene-divinylbenzene copolymer (for example, XAD-4)sorbent tube attached to a sampling pump. Macroreticularpolystyrene-divinylbenzene copolymer is referred to “sorbentresin” throughout this method. This test method is applicable topersonal or area sampling.
5、1.3 This test method is limited in sample duration by thecapacity of the sorbent tube for nicotine (about 300 g). Thistest method has been evaluated up to 24-h sample duration;however, samples are typically acquired for at least 1h(sometimes only 1 h). (2)1.4 For this test method, limits of detectio
6、n (LOD) andquantitation (LOQ) for nicotine at a sampling rate of 1.5 L/minare, respectively, 0.11 g/m3and 0.37 g/m3for 1-h sampleduration and 0.01 g/m3and 0.05 g/m3for 8-h sampleduration. The LOD and LOQ for 3-EP at a sampling rate of 1.5L/min are, respectively, 0.06 g/m3and 0.19 g/m3for 1-hsample d
7、uration and 0.01 g/m3and 0.02 g/m3for 8-h sampleduration (2). Both LOD and LOQ can be reduced by increasingthe sensitivity of the thermionic specific detector.1.5 UnitsThe values stated in SI units are to be regardedas standard. No other units of measurement are included in thisstandard.1.6 This sta
8、ndard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific precau-tionary in
9、formation is given in 13.6.2. Referenced Documents2.1 ASTM Standards:3D1356 Terminology Relating to Sampling and Analysis ofAtmospheresD1357 Practice for Planning the Sampling of the AmbientAtmosphereD3631 Test Methods for Measuring Surface AtmosphericPressureD5337 Practice for Flow Rate Adjustment
10、of Personal Sam-pling PumpsE260 Practice for Packed Column Gas ChromatographyE355 Practice for Gas Chromatography Terms and Relation-ships3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology D1356 and Practice E355.3.2 Definitions of Terms Specific to T
11、his Standard:3.2.1 environmental tobacco smoke (ETS)an aged, dilutecomposite of exhaled tobacco smoke (exhaled mainstreamsmoke) and smoke from tobacco products (sidestream smoke).3.2.2 nitrogen-phosphorus detector (NPD)a highly sensi-tive device selective for detection of nitrogen- and phosphorus-co
12、ntaining organic compounds.4. Summary of Test Method4.1 A known volume of air is drawn through a sorbentsampling tube containing resin to adsorb the nicotine and 3-EPpresent.4.2 The sorbent tube contents are transferred to a 2-mLautosampler vial, and the nicotine and 3-EP are desorbed withethyl acet
13、ate containing 0.01 % triethylamine and a knownquantity of quinoline, the internal standard.1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.Current edition approved March 1, 2017. Published March 20
14、17. Originallyapproved in 1990. Last previous edition approved in 2012 as D5075 01 (2012)1.DOI: 10.1520/D5075-01R17E01.2The boldface numbers in parentheses refer to a list of references at the end ofthe text.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Custome
15、r Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was develope
16、d in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14.3 An aliquot of the
17、desorbed sample is injected into a gaschromatograph equipped with a thermionic-specific (nitrogen-phosphorus) detector.4.4 The areas of the resulting nicotine and 3-EP peaks areeach divided by the area of the internal standard peak andcompared with area ratios obtained from the injection ofstandards
18、.5. Significance and Use5.1 In order to estimate ETS concentrations, there needs tobe a marker or tracer for ETS that is unique or highly specificto tobacco smoke, in sufficient concentrations in air to bemeasured easily at realistic smoking rates, and in constantproportion to the other components o
19、f ETS for a variety oftobacco blends and environmental conditions. Nicotine and3-ethenylpyridine have been used as tracers of the vapor phaseof ETS. Nicotine is the major alkaloid of tobacco and a majorconstituent of ETS. The determination of nicotine concentra-tion has often been used to estimate t
20、he concentration of ETS;however, due to its unpredictable decay kinetics, nicotine maynot be an ideal tracer. Because nicotine readily adsorbs tobuilding materials and room furnishings and is depleted fromETS at a rate faster than most other components, some havesuggested that nicotine concentration
21、s underestimate ETSconcentrations. Although this is true in many environmentsduring the generation of smoke, the converse is true inenvironments with a recent past history of smoking. Theadsorbed nicotine slowly desorbs over time, resulting in anoverestimation of ETS concentrations.Thus, measured co
22、ncen-trations of nicotine precisely assess only airborne nicotine andindicate only that smoking has taken place; they do notnecessarily indicate the presence, and certainly not theconcentrations, of other ETS constituents. 3-Ethenylpyridine,on the other hand, has been shown to track exactly the vapo
23、rphase of ETS as measured by CO and FID response (3).Itisfor these reasons that 3-ethenylpyridine may be a better tracerof ETS (1, 4, 5). The ETS at high concentrations is known tobe annoying and irritating to individuals, and concerns overpotential health effects have also been expressed. There is
24、adefinite need to have reliable methods for the estimation ofETS levels in order to evaluate its effect. The NIOSH haspreviously set a recommended exposure limit (REL) fornicotine in the workplace of 0.5 mg/m3.5.2 Studies show that more than 90 % of nicotine in indoorair is found in the vapor phase
25、(6, 7).The described test methodcollects vapor-phase nicotine quantitatively. Early studies onfreshly generated ETS indicated that some but not all of theparticulate phase was trapped on the resin (7). A more recentinvestigation of the trapping of particulate materials by sorbentbeds suggests that t
26、he trapping of the particles from indoor airmay be nearly quantitative (8). 3-Ethenylpyridine is foundexclusively in the vapor phase.5.3 Nicotine concentrations typically range from ND (notdetected) to 70 g/m3in various indoor environments withvalues usually at the lower end of this range (9). Becau
27、se suchlow concentrations of nicotine are often encountered, sophis-ticated analytical procedures and equipment are required forquantifying nicotine in indoor air. Other methods for thedetermination of nicotine in indoor air have also been reported(6, 10, 11, 12). 3-Ethenylpyridine concentrations ty
28、pically areabout one third the concentrations of nicotine in real-worldenvironments (13).6. Interferences6.1 Use of packed GC columns may result in readings lowerthan expected because nicotine can adsorb onto undeactivatedglass, metal, and solid support particles. Fused silica capillarycolumns and t
29、he modified extraction solvent prescribed herecan circumvent this problem.6.2 Quinoline (internal standard) is present in ETS at aconcentration approximately 1 % of that for nicotine and iscollected by the resin. If 10 g nicotine is collected on theresin, there will be sufficient quinoline present t
30、o cause adetectable bias in results (approximately 1 %). (For example,this quantity of nicotine would be collected if a nicotineconcentration of 167 g/m3was sampled at 1 L/min for 1 h.) Inthese cases, one of the following alternative procedures shouldbe followed:6.2.1 Quantitatively dilute the sampl
31、e with the same modi-fied solvent containing internal standard (described in 11.2)used to extract the original sample; that is, decrease the amountof quinoline (and also nicotine) present in the sample whilekeeping the quinoline concentration in the solvent constant. Toprevent significant interferen
32、ce, the nicotine concentration inthe most concentrated sample should be less than or equal tothe quinoline concentration in the solvent.6.2.2 Use an alternate internal standard N-ethylnornico-tine is recommended (14).7. Apparatus7.1 Sample Collection:7.1.1 Sorbent TubeGlass tube with both ends flame
33、-sealed, approximately 7 cm long with 6-mm outside diameterand 4-mm inside diameter, containing one section of 120 mg of20/40 mesh resin. A glass wool plug is located at the front end(inlet) and back end of the tube.The glass wool plug at the inletend of the tube is held in place with a metal locksp
34、ring.7.1.2 Tube Holder, with clip attachment for attaching tube toclothing or objects.7.1.3 Tube Breaker, to break sealed ends from sample tubes.7.1.4 NIOSH-approved Plastic Caps, for capping tubes aftersampling.7.1.5 Barometer and Thermometer, for taking pressure andtemperature readings at the samp
35、ling site (optional).7.1.6 Bubble Flowmeter, for sample pump calibration.7.1.7 Personal Sampling Pump, portable constant-flow sam-pling pump calibrated for the flow rate desired (up to 1.5L/min).7.2 Analytical System:7.2.1 Gas Chromatograph, with a nitrogen-phosphorus(thermionic) detector and autosa
36、mpler.7.2.2 GC ColumnA 30-m by 0.32-mm inside diameterfused silica capillary column, coated with a 1.0-m film of 5 %phenyl methylpolysiloxane (DB-5).D5075 01 (2017)127.2.3 Chromatography Data Acquisition System, for mea-suring peak areas electronically.7.2.4 Sample Containers, borosilicate glass aut
37、osamplervials, 2-mL capacity, with PTFE-lined septum closures.7.2.5 Dispensing Pipets, 1.25-mL.7.2.6 Triangular File, for scoring and breaking open sampletubes.7.2.7 Forceps, for assisting transfer of sorbent tube contentsfrom tube to autosampler vial.7.2.8 Glass Wool Removal Tool, for assisting tra
38、nsfer ofsorbent tube contents from tube to autosampler vial.7.2.9 Wrist-action Shaking Device, for solvent extraction.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifica
39、tions of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available. Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.8.2 Ethy
40、l Acetate, chromatographic quality.8.3 Quinoline (internal standard), 99+ %.8.4 Triethylamine, 99+ %.8.5 Nicotine, 99+ %.8.6 4-Ethenylpyridine (4-EP), 95 %, commercially avail-able isomer of 3-ethenylpyridine.8.7 Helium Cylinders, for carrier or detector makeup gas, orboth, 99.995 % grade.8.8 Hydrog
41、en Cylinders, for detector gas, 99.995 % grade.8.9 Air, for detector gas (5 % of tube contents found inbackup resin section) can occur after collecting approximately300 g nicotine in a single tube. A shorter sampling time isnecessary if sample concentration and duration of samplingsuggest a breakthr
42、ough occurrence.11. Procedure11.1 Sorbent Tube AnalysisThe analytical procedure fornicotine and 3-EP is performed by extracting the sorbent resinwith modified ethyl acetate solvent followed by GC/NPDanalysis. Ethyl acetate extracts nicotine and 3-EP from thesorbent resin, but the solvent is modified
43、 with 0.01 % v/vtriethylamine to prevent any adsorption of nicotine on the glasswalls of the vials (14). The solvent also contains the internalstandard quinoline, at a concentration of approximately 8g/mL. Solvent henceforth will refer to this modified ethylacetate solvent.11.2 Preparation of Modifi
44、ed Ethyl Acetate Solvent:11.2.1 To a previously unopened 4-L bottle of ethyl acetate,add 0.5 mL triethylamine and 30 L quinoline. Shake vigor-ously to mix.11.2.1.1 To a separate freshly opened 4-L bottle of ethylacetate, add 0.5 mL triethylamine; shake vigorously to mix.Use modified solvent containi
45、ng no internal standard onlywhen specifically called for in the procedure.11.2.2 Store the modified ethyl acetate solvent containingquinoline at 4C or less when not in use. Allow the solvent toreach room temperature before using it to prepare standardsolutions or samples.11.2.3 Prepare fresh modifie
46、d solvent as needed. Deteriora-tion of the modified solvent has not been observed, and nodefinitive time interval has been established for its replace-ment; however, storage and use for more than 12 months is notrecommended.NOTE 3In order to keep the amount of internal standard constant forboth stan
47、dards and samples, the same batch of modified solvent that isused to prepare standard solutions must be used to extract samples.Therefore, whenever a new batch of modified solvent is prepared, a newbatch of standard solutions must also be prepared. Otherwise, if standardsand samples contain differen
48、t amounts of internal standard, the exactamounts in both solutions must be known precisely, and the regression andequations in 11.6.1 and 12.1 must be modified to reflect the differentinternal standard concentrations.11.3 Preparation of Standard Solutions:11.3.1 Clean all volumetric flasks and screw
49、-cap jars usedfor the preparation and storage of standard solutions withdetergent, thoroughly rinse with tap water followed by distilledwater followed by ethyl acetate containing only 0.01 % trieth-ylamine with no quinoline, and allow to air dry.11.3.2 Prepare a primary standard of nicotine containing400 g/mL by weighing 100 mg of nicotine directly into a250-mL volumetric flask, diluting to volume with solvent, andshaking to mix. Prepare a primary standard of 4-EP containing500 g/mL by weighing 100 mg of 4-EP into a 200-mLvolumetric flask, dilutin
